一种以含硅藻土的复合材料为介质的支撑液液萃取柱的制备及其应用

Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material

以含硅藻土的复合材料为支撑介质,开发了一种独特的支撑液液萃取柱;以一系列酸性、碱性和中性水溶液样品为模型化合物,结合高效液相色谱法(HPLC)对该萃取柱进行了系统评价,同时将其用于复杂基质样品的分析。结果表明:经该支撑液液萃取柱预处理的苯甲酸、对硝基苯胺和对羟基苯甲酸甲酯水溶液的萃取回收率分别为90.6%、98.1%和97.7%,远超过对应样品经传统液液萃取法处理后的回收率(分别为71.9%、81.9%和83.9%)。对于复杂基质样品的分析,如雪碧中的防腐剂苯甲酸以及牛血清中的中性药物醋酸地塞米松、碱性药物马来酸氯苯那敏及酸性药物吲哚美辛等,样品的加标回收率均在80%和110%之间,相对标准偏差(RSD)均小于15%,符合生物样品的分析要求,且未出现传统液液萃取技术中常见的问题(如乳化现象)。所开发的支撑液液萃取柱具有快速、简单、耐受性好、易于实现自动化和高通量的特点,具有广泛的应用前景。

A rapid and special supported liquid-liquid extraction（SLE） column was developed with a composite diatomite material.The SLE column was evaluated by high performance liquid chromatography（HPLC） with acidic,neutral and alkaline compounds dissolved in water.Furthermore,some real complex samples were also analyzed by HPLC with the SLE method.The recoveries of benzoic acid（acidic）,p-nitroaniline（alkaline） and 4-hydroxy-benzoic methyl ester（neutral） treated by the SLE column were 90.6%,98.1% and 97.7%.However,the recoveries of the three compounds treated by traditional liquid-liquid extraction（LLE） method were 71.9%,81.9% and 83.9%.The results showed that the SLE technique had higher recoveries than the traditional LLE method.The spiked recoveries of the complex samples,such as benzoic acid in Sprite and dexamethasone acetate,chlorphenamine maleate,indomethacin in bovine serum,were between 80% and 110% and the relative standard deviations（RSDs） were less than 15%.For biological specimen,the results could be accepted.Meantime,many disadvantages associated with traditional LLE method,such as emulsion formation,didn＇t occur using SLE column.The SLE column technique is a good sample preparation method with many advantages,such as rapid,simple,robust,easily automated,high recovery and high-throughput,which would be widely used in the future.